CN111099706A - Method for recycling tantalum in acid-containing waste liquid - Google Patents
Method for recycling tantalum in acid-containing waste liquid Download PDFInfo
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- CN111099706A CN111099706A CN201911277210.4A CN201911277210A CN111099706A CN 111099706 A CN111099706 A CN 111099706A CN 201911277210 A CN201911277210 A CN 201911277210A CN 111099706 A CN111099706 A CN 111099706A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/101—Sulfur compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The invention relates to a method for recovering and treating tantalum in tantalum-containing acidic waste liquid, which comprises the following steps: (1) adding sodium hydroxide into the tantalum-containing acidic waste liquid to react to generate tantalate precipitate; adding an inorganic flocculant for coagulation after the precipitate is generated, and performing solid-liquid separation to obtain a tantalate precipitate and a primary treatment waste liquid; (2) adding sodium hydroxide into the primary treatment waste liquid to adjust the pH, adding calcium salt after adjustment to react to generate fluoride salt precipitate, adding an inorganic flocculant, an organic flocculant and a coagulant to perform coagulation, and performing solid-liquid separation to obtain fluoride salt precipitate and secondary treatment waste liquid; (3) after the secondary treatment waste liquid is subjected to composite filtration,adding pH regulator to regulate pH and discharging. The method for recovering and treating the acid waste liquid containing tantalum can use NaTaO as tantalum ions in the waste liquid3The recovery rate can reach more than 98 percent, the purity can reach more than 95 percent, and the treated waste liquid completely reaches the standard and is discharged; and the process is simple, the treatment cost is low, and the method is safe and efficient.
Description
Technical Field
The invention belongs to the technical field of metal smelting waste liquid treatment, and particularly relates to a method for recovering and treating tantalum in tantalum-containing acidic waste liquid.
Background
Tantalum metal is used as a rare precious metal, raw ores of the tantalum metal are distributed and dispersed, and the storage capacity and the grade are not high, tantalum is used as a black gray transition metal, coexists with niobium in niobium tantalite, has stable chemical properties, has a high melting point (the melting point is 2996 ℃), and is the third most refractory metal which is second to tungsten and rhenium; the cold workability is good, corrosion-resistant, and widely applied to the high-technology industrial fields including electronics, precision ceramics and precision glass industry, electro-acoustic optical devices, hard alloy, aerospace and electronic energy industry, biomedical engineering, superconducting industry, special steel and the like.
Tantalum-niobium hydrometallurgy in the production process of tantalum-niobium hydrometallurgy, hydrofluoric acid (HF) and concentrated sulfuric acid (H) are mainly used2SO4) Decomposing the tantalum-niobium ore equally, filtering, and then extracting and separating the filtrate by using an extracting agent to obtain potassium fluotantalate, tantalum oxide and niobium oxide products. A large amount of acidic waste liquid, such as ore extraction raffinate and acid pickling raffinate, can be generated in the tantalum-niobium hydrometallurgy production process; the acid wastewater contains a large amount of fluoride ions, sulfate ions and metal ions, wherein the tantalum ions are TaF in liquid state6 2-Is present in the acidic waste liquid. At present, liquid ammonia is mainly adopted in China to neutralize acid waste liquid and tantalum ions in the acid waste liquid are recovered; however, the liquid ammonia neutralization method has obvious process defects, mainly liquid ammonia belongs to dangerous chemicals, is improper to operate and is easy to cause poisoning and fire, and after tantalum metal compounds are recovered, tail liquid contains a large amount of ammonia nitrogen, so that the treatment cost is high, the standard treatment and discharge process of the ammonia nitrogen in the later stage of tantalum metal in waste liquid is seriously restricted, and the recycling of the large-investment metal compounds is realized. How to ensure the efficient recovery and standard discharge of valuable metals in the acid wastewater in the tantalum-niobium hydrometallurgy process is the key point of attention of tantalum-niobium hydrometallurgy enterprises. At present, there are also many researches on the treatment of acid waste liquid from tantalum-niobium hydrometallurgy.
For example, the patent with the publication number of CN106865724A discloses a method for treating raffinate and comprehensive wastewater from tantalum-niobium hydrometallurgy; the method comprises the following operations: adjusting pH to 7-7.5 with ammonia gas or ammonia water to form precipitate, and separating for the first time; adjusting pH to 5-6 with sulfuric acid, forming precipitate in the presence of aluminum salt and sodium salt, and separating for the second time; adjusting pH to above 12 with calcium hydroxide, and separating precipitate to obtain treated solution. Valuable substances in the extraction residual liquid are separated and recovered in a precipitation form to realize sewage treatment, so that resource reutilization is realized; meanwhile, the treatment amount is reduced, and the treatment is thorough. The patent does not realize the recovery of tantalum metal in the waste liquid, and ammonia nitrogen impurities are introduced in the treatment process, so that the treatment difficulty of the acidic waste liquid is increased.
Also, for example, patent publication No. CN110255503A discloses a method for treating raffinate of tantalum-niobium extraction: s1) carrying out evaporative crystallization on the residual liquid of the tantalum-niobium extraction to respectively obtain hydrogen fluoride gas and crystallization mother liquor; the concentration of sulfuric acid in the tantalum-niobium extraction raffinate is not lower than 400g/L, and the concentration of hydrofluoric acid is not lower than 60 g/L; the concentration of sulfuric acid in the crystallization mother liquor is not lower than 1000 g/L; s2) mixing the crystallization mother liquor obtained in the step S1) with a precipitator, reacting, and carrying out solid-liquid separation to obtain a sulfuric acid-containing solution and sediments; the precipitant is alkali metal salt. The patent adopts an evaporative crystallization method to recover hydrofluoric acid and sulfuric acid in the acidic waste liquid, so that the requirement on equipment is high and the treatment cost is high; and the recovery of tantalum metal in the waste liquid is realized.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a method for recovering and treating tantalum in tantalum-containing acidic waste liquid, which is realized by the following technical scheme:
a method for recovering and treating tantalum in tantalum-containing acidic waste liquid comprises the following steps:
(1) adding sodium hydroxide into the tantalum-containing acidic waste liquid to react to generate tantalate precipitate; adding an inorganic flocculant for coagulation after the precipitate is generated, and performing solid-liquid separation to obtain a tantalate precipitate and a primary treatment waste liquid;
(2) adding sodium hydroxide into the primary treatment waste liquid to adjust the pH value of the primary treatment waste liquid to 8-10, adding calcium salt after adjustment to react to generate fluoride salt precipitate, adding an inorganic flocculant, an organic flocculant and a coagulant to perform coagulation, and performing solid-liquid separation to obtain fluoride salt precipitate and secondary treatment waste liquid;
(3) and (4) after the secondary treatment waste liquid is subjected to composite filtration, adding a pH regulator to regulate the pH value to 6-9, and then discharging the waste liquid after reaching the standard.
Preferably, in the step (1), sodium hydroxide is added to adjust the pH value of the tantalum-containing acidic waste liquid to be more than 11; the inorganic flocculant is polyaluminium sulfate, and the addition amount of the inorganic flocculant is 0.7-1% of the waste liquid amount.
Preferably, in the step (2), the calcium salt is calcium chloride, and the addition amount is 2-3% of the waste liquid amount.
Preferably, in the step (2), the inorganic flocculant is polyaluminium sulfate, the organic flocculant is polyacrylamide, and the coagulant is polyaluminium chloride.
Preferably, in the step (2), the addition amount of the inorganic flocculant is 0.7-1% of the waste liquid amount, the addition amount of the organic flocculant is 0.1-0.2% of the waste liquid amount, and the addition amount of the coagulant is 0.7-1% of the waste liquid amount.
Preferably, in the step (3), the pH regulator is sulfuric acid.
Preferably, the solid-liquid separation adopts a dark flow diaphragm type solid-liquid separator.
Preferably, the composite filter adopts an activated carbon-quartz sand multi-medium filter.
The invention has the beneficial effects that:
the acid waste liquid containing tantalum produced by tantalum-niobium hydrometallurgy contains metal ions such as tantalum and the like and a large amount of fluorine ions and sulfate ions; TaF of tantalum in acidic waste liquid6 2-Exist in the form of (1). The method adopts excessive sodium hydroxide and tantalum-containing acidic waste liquid to react firstly, and then Na is added+In a rich environment, TaF6 2-Can react to generate insoluble NaTaO3Precipitating, and then polymerizing by using a polyaluminium sulfate flocculating agent, so that the recovery of tantalum in the tantalum-containing acidic waste liquid can be realized; then adding calcium salt into the primary treated waste liquid to react under the alkaline condition, precipitating out fluoride ions in the waste liquid in the form of calcium fluoride, and then adding an organic flocculantThe inorganic flocculant and the coagulant are polymerized and then are subjected to solid-liquid separation, so that fluorine ions in the waste liquid can be removed; finally, the secondary treatment waste liquid is treated by a multi-medium filter, so that residual impurities in the secondary treatment waste liquid can be effectively removed, and the treated waste liquid completely reaches the standard and is discharged.
The method for recovering and treating the acid waste liquid containing tantalum can use NaTaO as tantalum ions in the waste liquid3The recovery rate of tantalum can reach more than 98 percent, and NaTaO3The purity of the product can reach more than 95 percent; the fluorine content of the treated waste liquid is lower than 10mg/L, and the waste liquid completely reaches the standard and is discharged; and the process is simple, the treatment cost is low, and the method is safe and efficient.
Detailed Description
The technical solution of the present invention is further defined below with reference to the specific embodiments, but the scope of the claims is not limited to the description.
Example 1
Treating raw materials: the acid waste liquid containing tantalum produced by 60L tantalum-niobium hydrometallurgy contains 13.17g/L tantalum ions, 5.01g/L fluorine ions and 0.06% ferrous nitrate.
The recovery processing method comprises the following steps:
(1) adding sodium hydroxide into the acid waste liquid containing tantalum to adjust the pH value to be more than 11, and reacting to generate NaTaO3Precipitating; adding polyaluminium sulfate with waste liquid amount of 0.7% after precipitation is generated for coagulation, and performing solid-liquid separation by a dark flow diaphragm type solid-liquid separator to obtain NaTaO3Precipitating and primary treating waste liquid;
(2) adding sodium hydroxide into the primary treated waste liquid to adjust the pH value to 8-10, adding calcium chloride with the waste liquid amount being 2% to react to generate calcium fluoride precipitate, adding polyaluminum sulfate with the waste liquid amount being 0.7%, polyacrylamide with the waste liquid amount being 0.2% and polyaluminum chloride with the waste liquid amount being 0.7% to perform condensation, and performing solid-liquid separation by adopting a dark current diaphragm type solid-liquid separator to obtain calcium fluoride precipitate and secondary treated waste liquid;
(3) and (3) performing composite filtration on the secondary treatment waste liquid by using an activated carbon-quartz sand multi-medium filter, adding sulfuric acid to adjust the pH value to 6-9, and discharging the waste liquid after reaching the standard.
As described aboveAfter 60L of acid waste liquid containing tantalum is treated, 1.12kg of NaTaO can be obtained3,NaTaO3The purity of (A) was 96.1%, and the recovery rate of tantalum ions was 98.17%. The treated waste liquid is detected, F-The content is lower than 10mg/L, and the national third-level emission standard is completely achieved.
Example 2
Treating raw materials: 200L of acid waste liquid containing tantalum produced by tantalum-niobium hydrometallurgy, 13.21g/L of tantalum ions, 4.97g/L of fluorine ions and 2 percent of magnesium nitrate.
The recovery processing method comprises the following steps:
(1) adding sodium hydroxide into the acid waste liquid containing tantalum to the pH value of more than 11, and reacting to generate NaTaO3Precipitating; adding inorganic flocculant with waste liquid amount of 0.8% for coagulation after the precipitate is generated, and performing solid-liquid separation by a dark flow diaphragm type solid-liquid separator to obtain NaTaO3Precipitating and primary treating waste liquid;
(2) adding sodium hydroxide into the primary treated waste liquid to adjust the pH value to 8-10, adding calcium chloride with the waste liquid amount of 2.4% after adjustment to react to generate calcium fluoride precipitate, adding polyaluminium sulfate with the waste liquid amount of 0.8%, polyacrylamide with the waste liquid amount of 0.15% and polyaluminium chloride with the waste liquid amount of 0.8% for condensation, and then carrying out solid-liquid separation by adopting a dark current diaphragm type solid-liquid separator to obtain calcium fluoride precipitate and secondary treated waste liquid;
(3) and (3) performing composite filtration on the secondary treatment waste liquid by using an activated carbon-quartz sand multi-medium filter, adding a pH regulator to regulate the pH value to 6-9, and discharging the secondary treatment waste liquid after reaching the standard.
After the 200L of acid waste liquid containing tantalum is treated, 3.81kg of NaTaO can be obtained3,NaTaO3The purity of (A) was 95.0%, and the recovery rate of tantalum ions was 98.42%. The treated waste liquid is detected, F-The content is lower than 10mg/L, and the national third-level emission standard is completely achieved.
Example 3
Treating raw materials: the acid waste liquid containing tantalum produced by 25L tantalum-niobium hydrometallurgy contains 13.15g/L tantalum ions, 5.06g/L fluorine ions and 0.1% ferrous nitrate.
The recovery processing method comprises the following steps:
(1) to the above tantalum-containingAdding sodium hydroxide into the acidic waste liquid to adjust the pH value to be more than 11, and reacting to generate NaTaO3Precipitating; adding polyaluminium sulfate with waste liquid amount of 1% to coagulate after precipitation, and performing solid-liquid separation with a dark flow diaphragm type solid-liquid separator to obtain NaTaO3Precipitating and primary treating waste liquid;
(2) adding sodium hydroxide into the primary treated waste liquid to adjust the pH value of the primary treated waste liquid to 8-10, adding calcium chloride with the waste liquid amount being 3% to react to generate calcium fluoride precipitate, adding polyaluminum sulfate with the waste liquid amount being 1%, polyacrylamide with the waste liquid amount being 0.2% and polyaluminum chloride with the waste liquid amount being 1% to perform condensation, and performing solid-liquid separation by adopting a dark flow diaphragm type solid-liquid separator to obtain calcium fluoride precipitate and secondary treated waste liquid;
(3) and (3) performing composite filtration on the secondary treatment waste liquid by using an activated carbon-quartz sand multi-medium filter, adding a pH regulator to regulate the pH value to 6-9, and discharging the secondary treatment waste liquid after reaching the standard.
After the 25L of acid waste liquid containing tantalum is treated, 0.47kg of NaTaO can be obtained3,NaTaO3The purity of (A) was 95.6%, and the recovery rate of tantalum ions was 98.32%. The treated waste liquid is detected, F-The content is lower than 10mg/L, and the national third-level emission standard is completely achieved.
Example 4
Treating raw materials: the acid waste liquid containing tantalum produced by 300L tantalum-niobium hydrometallurgy contains 13.19g/L tantalum ions, 5.12g/L fluorine ions and 2% of magnesium nitrate.
The recovery processing method comprises the following steps:
(1) adding sodium hydroxide into the acid waste liquid containing tantalum to react to generate NaTaO3Precipitating; adding inorganic flocculant with waste liquid amount of 0.7% for coagulation after the precipitate is generated, and performing solid-liquid separation by a dark flow diaphragm type solid-liquid separator to obtain NaTaO3Precipitating and primary treating waste liquid;
(2) adding sodium hydroxide into the primary treated waste liquid to adjust the pH value to 8-10, adding calcium chloride with the waste liquid amount being 3% to react to generate calcium fluoride precipitate, adding polyaluminum sulfate with the waste liquid amount being 0.8%, polyacrylamide with the waste liquid amount being 0.2% and polyaluminum chloride with the waste liquid amount being 1% to perform condensation, and performing solid-liquid separation by adopting a dark flow diaphragm type solid-liquid separator to obtain calcium fluoride precipitate and secondary treated waste liquid;
(3) and (3) performing composite filtration on the secondary treatment waste liquid by using an activated carbon-quartz sand multi-medium filter, adding a pH regulator to regulate the pH value to 6-9, and discharging the secondary treatment waste liquid after reaching the standard.
After the 300L of acid waste liquid containing tantalum is treated, 5.69kg of NaTaO can be obtained3,NaTaO3The purity of (A) was 95.4%, and the recovery rate of tantalum ions was 98.53%. The treated waste liquid is detected, F-The content is lower than 10mg/L, and the national third-level emission standard is completely achieved.
It should be noted that the above examples and test examples are only for further illustration and understanding of the technical solutions of the present invention, and are not to be construed as further limitations of the technical solutions of the present invention, and the invention which does not highlight essential features and significant advances made by those skilled in the art still belongs to the protection scope of the present invention.
Claims (8)
1. The method for recycling tantalum in tantalum-containing acidic waste liquid is characterized by comprising the following steps:
(1) adding sodium hydroxide into the tantalum-containing acidic waste liquid to react to generate tantalate precipitate; adding an inorganic flocculant for coagulation after the precipitate is generated, and performing solid-liquid separation to obtain a tantalate precipitate and a primary treatment waste liquid;
(2) adding sodium hydroxide into the primary treatment waste liquid to adjust the pH value of the primary treatment waste liquid to 8-10, adding calcium salt after adjustment to react to generate fluoride salt precipitate, adding an inorganic flocculant, an organic flocculant and a coagulant to perform coagulation, and performing solid-liquid separation to obtain fluoride salt precipitate and secondary treatment waste liquid;
(3) and (4) performing composite filtration on the secondary treatment waste liquid, adding a pH regulator to regulate the pH value to 6-9, and discharging the secondary treatment waste liquid after reaching the standard.
2. The method for recovering and treating tantalum in tantalum-containing acidic waste liquid as claimed in claim 1, wherein in step (1), sodium hydroxide is added to adjust the pH of tantalum-containing acidic waste liquid to above 11; the inorganic flocculant is polyaluminium sulfate, and the addition amount of the inorganic flocculant is 0.7-1% of the waste liquid amount.
3. The method for recovering and treating tantalum in the tantalum-containing acidic waste liquid as claimed in claim 1, wherein in the step (2), the calcium salt is calcium chloride, and the addition amount is 2-3% of the waste liquid amount.
4. The method according to claim 1, wherein in the step (2), the inorganic flocculant is polyaluminium sulfate, the organic flocculant is polyacrylamide, and the coagulant is polyaluminium chloride.
5. The method according to claim 1, wherein in the step (2), the amount of the inorganic flocculant added is 0.7 to 1% of the amount of the waste liquid, the amount of the organic flocculant added is 0.1 to 0.2% of the amount of the waste liquid, and the amount of the coagulant added is 0.7 to 1% of the amount of the waste liquid.
6. The method according to claim 1, wherein in step (3), the pH regulator is sulfuric acid.
7. The method according to claim 1, wherein the solid-liquid separation is performed by a solid-liquid separator of a non-flowing diaphragm type.
8. The method for recycling tantalum in tantalum-containing acidic waste liquid according to claim 1, wherein the composite filtration is performed by using a coconut shell activated carbon-quartz sand multi-media filter.
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2019
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CN107162253A (en) * | 2017-05-04 | 2017-09-15 | 常熟三爱富中昊化工新材料有限公司 | A kind of processing method of fluoride waste |
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